Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 626323' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H70 O7 Si4 Ti2' _chemical_formula_weight 1207.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.787(3) _cell_length_b 15.713(3) _cell_length_c 20.904(4) _cell_angle_alpha 69.76(2) _cell_angle_beta 79.648(10) _cell_angle_gamma 78.22(2) _cell_volume 3231.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.372 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_correction_T_max 0.836 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'four circle diffractometer Nonius-Mach3' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 13552 _diffrn_reflns_av_R_equivalents 0.1132 _diffrn_reflns_av_sigmaI/netI 0.4337 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13175 _reflns_number_gt 5320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (control program)' _computing_cell_refinement 'Nonius (control program)' _computing_data_reduction 'XRAY80 (Stewart, 1976)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13175 _refine_ls_number_parameters 740 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3409 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti11 Ti 0.48684(10) 0.16943(7) 0.25579(6) 0.0416(4) Uani 1 1 d . . . Si11 Si 0.41083(18) 0.29576(13) 0.10704(10) 0.0467(5) Uani 1 1 d . . . Si12 Si 0.36287(19) 0.38208(13) 0.21913(11) 0.0510(6) Uani 1 1 d . . . O11 O 0.4564(4) 0.2006(2) 0.1656(2) 0.0428(11) Uani 1 1 d . . . O12 O 0.4100(4) 0.2803(3) 0.2706(2) 0.0464(12) Uani 1 1 d . . . O13 O 0.3783(4) 0.3782(3) 0.1415(2) 0.0501(12) Uani 1 1 d . . . Ti21 Ti 0.28181(10) -0.00234(8) 0.32735(6) 0.0399(4) Uani 1 1 d . . . Si21 Si 0.34470(19) -0.11859(14) 0.22312(10) 0.0524(6) Uani 1 1 d . . . Si22 Si 0.42141(19) -0.21200(13) 0.36550(10) 0.0497(6) Uani 1 1 d . . . O21 O 0.3667(3) -0.1139(2) 0.37795(18) 0.0410(11) Uani 1 1 d . . . O22 O 0.2907(4) -0.0291(3) 0.2471(2) 0.0476(12) Uani 1 1 d . . . O23 O 0.4014(4) -0.2033(3) 0.2872(2) 0.0563(13) Uani 1 1 d . . . O1 O 0.3846(4) 0.0836(3) 0.3054(2) 0.0483(12) Uani 1 1 d . . . C10 C 0.6382(6) 0.0790(5) 0.3302(4) 0.0508(19) Uani 1 1 d . . . C11 C 0.6697(6) 0.0565(4) 0.2696(4) 0.0445(18) Uani 1 1 d . . . C12 C 0.7054(5) 0.1332(5) 0.2152(4) 0.0450(18) Uani 1 1 d . . . C13 C 0.6964(6) 0.2048(5) 0.2427(4) 0.053(2) Uani 1 1 d . . . C14 C 0.6553(6) 0.1715(5) 0.3138(4) 0.053(2) Uani 1 1 d . . . C15 C 0.5989(6) 0.0153(5) 0.4001(3) 0.073(2) Uani 1 1 d . . . H15A H 0.5234 -0.0074 0.3990 0.110 Uiso 1 1 calc R . . H15B H 0.5817 0.0479 0.4328 0.110 Uiso 1 1 calc R . . H15C H 0.6664 -0.0353 0.4132 0.110 Uiso 1 1 calc R . . C16 C 0.6704(6) -0.0374(4) 0.2630(4) 0.068(2) Uani 1 1 d . . . H16A H 0.5904 -0.0582 0.2839 0.102 Uiso 1 1 calc R . . H16B H 0.7384 -0.0805 0.2857 0.102 Uiso 1 1 calc R . . H16C H 0.6828 -0.0327 0.2153 0.102 Uiso 1 1 calc R . . C17 C 0.7521(6) 0.1359(4) 0.1435(3) 0.067(2) Uani 1 1 d . . . H17A H 0.8315 0.0953 0.1425 0.101 Uiso 1 1 calc R . . H17B H 0.7645 0.1973 0.1159 0.101 Uiso 1 1 calc R . . H17C H 0.6905 0.1168 0.1255 0.101 Uiso 1 1 calc R . . C18 C 0.7355(6) 0.2983(4) 0.2041(4) 0.075(2) Uani 1 1 d . . . H18A H 0.8266 0.2918 0.1937 0.113 Uiso 1 1 calc R . . H18B H 0.7077 0.3376 0.2320 0.113 Uiso 1 1 calc R . . H18C H 0.6969 0.3248 0.1622 0.113 Uiso 1 1 calc R . . C19 C 0.6362(7) 0.2238(5) 0.3632(4) 0.090(3) Uani 1 1 d . . . H19A H 0.5662 0.2054 0.3976 0.135 Uiso 1 1 calc R . . H19B H 0.6180 0.2883 0.3391 0.135 Uiso 1 1 calc R . . H19C H 0.7123 0.2114 0.3848 0.135 Uiso 1 1 calc R . . C20 C 0.2676(6) 0.2831(5) 0.0754(3) 0.0499(19) Uani 1 1 d . . . C21 C 0.2113(7) 0.2056(5) 0.1006(4) 0.064(2) Uani 1 1 d . . . H21 H 0.2457 0.1563 0.1357 0.077 Uiso 1 1 calc . . . C22 C 0.1052(8) 0.1978(6) 0.0756(5) 0.082(3) Uani 1 1 d . . . H22 H 0.0712 0.1433 0.0927 0.098 Uiso 1 1 calc . . . C23 C 0.0508(8) 0.2702(8) 0.0260(5) 0.090(3) Uani 1 1 d . . . H23 H -0.0220 0.2661 0.0098 0.108 Uiso 1 1 calc . . . C24 C 0.1034(9) 0.3486(7) 0.0000(5) 0.100(3) Uani 1 1 d . . . H24 H 0.0661 0.3982 -0.0340 0.119 Uiso 1 1 calc . . . C25 C 0.2116(8) 0.3558(5) 0.0234(4) 0.080(3) Uani 1 1 d . . . H25 H 0.2473 0.4095 0.0044 0.096 Uiso 1 1 calc . . . C30 C 0.5393(6) 0.3229(5) 0.0346(3) 0.0490(19) Uani 1 1 d . . . C31 C 0.5708(7) 0.2709(5) -0.0086(4) 0.062(2) Uani 1 1 d . . . H31 H 0.5223 0.2257 -0.0030 0.074 Uiso 1 1 calc . . . C32 C 0.6716(8) 0.2835(6) -0.0597(4) 0.076(2) Uani 1 1 d . . . H32 H 0.6890 0.2487 -0.0892 0.092 Uiso 1 1 calc . . . C33 C 0.7462(7) 0.3480(6) -0.0667(4) 0.075(3) Uani 1 1 d . . . H33 H 0.8173 0.3549 -0.0996 0.090 Uiso 1 1 calc . . . C34 C 0.7162(7) 0.4016(5) -0.0256(4) 0.069(2) Uani 1 1 d . . . H34 H 0.7645 0.4473 -0.0320 0.082 Uiso 1 1 calc . . . C35 C 0.6147(7) 0.3891(5) 0.0257(4) 0.057(2) Uani 1 1 d . . . H35 H 0.5967 0.4250 0.0544 0.069 Uiso 1 1 calc . . . C40 C 0.1921(7) 0.4211(4) 0.2438(4) 0.056(2) Uani 1 1 d . . . C41 C 0.1007(8) 0.4433(5) 0.2001(4) 0.079(3) Uani 1 1 d . . . H41 H 0.1241 0.4400 0.1559 0.095 Uiso 1 1 calc . . . C42 C -0.0263(9) 0.4705(6) 0.2213(6) 0.101(3) Uani 1 1 d . . . H42 H -0.0883 0.4831 0.1923 0.121 Uiso 1 1 calc . . . C43 C -0.0591(10) 0.4786(7) 0.2861(7) 0.112(4) Uani 1 1 d . . . H43 H -0.1429 0.5005 0.2995 0.134 Uiso 1 1 calc . . . C44 C 0.0277(11) 0.4554(8) 0.3294(6) 0.132(4) Uani 1 1 d . . . H44 H 0.0036 0.4585 0.3736 0.159 Uiso 1 1 calc . . . C45 C 0.1529(9) 0.4269(6) 0.3089(5) 0.099(3) Uani 1 1 d . . . H45 H 0.2127 0.4112 0.3397 0.119 Uiso 1 1 calc . . . C50 C 0.4625(6) 0.4641(4) 0.2204(4) 0.052(2) Uani 1 1 d . . . C51 C 0.5182(7) 0.5233(5) 0.1605(4) 0.060(2) Uani 1 1 d . . . H51 H 0.5019 0.5240 0.1181 0.072 Uiso 1 1 calc . . . C52 C 0.5963(8) 0.5804(5) 0.1629(5) 0.078(3) Uani 1 1 d . . . H52 H 0.6347 0.6178 0.1223 0.094 Uiso 1 1 calc . . . C53 C 0.6179(9) 0.5829(6) 0.2240(6) 0.089(3) Uani 1 1 d . . . H53 H 0.6706 0.6226 0.2244 0.106 Uiso 1 1 calc . . . C54 C 0.5658(9) 0.5298(6) 0.2839(5) 0.083(3) Uani 1 1 d . . . H54 H 0.5815 0.5324 0.3255 0.100 Uiso 1 1 calc . . . C55 C 0.4866(8) 0.4702(5) 0.2819(4) 0.075(2) Uani 1 1 d . . . H55 H 0.4489 0.4335 0.3231 0.089 Uiso 1 1 calc . . . C60 C 0.1361(6) -0.0127(5) 0.4276(4) 0.053(2) Uani 1 1 d . . . C61 C 0.0808(6) -0.0391(5) 0.3838(4) 0.052(2) Uani 1 1 d . . . C62 C 0.0589(6) 0.0369(5) 0.3250(4) 0.0475(18) Uani 1 1 d . . . C63 C 0.1031(6) 0.1098(5) 0.3329(4) 0.055(2) Uani 1 1 d . . . C64 C 0.1487(6) 0.0809(5) 0.3965(4) 0.055(2) Uani 1 1 d . . . C65 C 0.1717(7) -0.0727(5) 0.4976(3) 0.077(2) Uani 1 1 d . . . H65A H 0.1424 -0.1306 0.5095 0.116 Uiso 1 1 calc R . . H65B H 0.1327 -0.0431 0.5310 0.116 Uiso 1 1 calc R . . H65C H 0.2627 -0.0828 0.4968 0.116 Uiso 1 1 calc R . . C66 C 0.0449(6) -0.1319(5) 0.3958(4) 0.079(3) Uani 1 1 d . . . H66A H 0.0676 -0.1476 0.3543 0.118 Uiso 1 1 calc R . . H66B H -0.0454 -0.1297 0.4091 0.118 Uiso 1 1 calc R . . H66C H 0.0896 -0.1773 0.4316 0.118 Uiso 1 1 calc R . . C67 C -0.0020(6) 0.0402(5) 0.2646(4) 0.088(3) Uani 1 1 d . . . H67A H 0.0038 -0.0210 0.2633 0.132 Uiso 1 1 calc R . . H67B H 0.0415 0.0764 0.2229 0.132 Uiso 1 1 calc R . . H67C H -0.0900 0.0672 0.2691 0.132 Uiso 1 1 calc R . . C68 C 0.0927(7) 0.2077(5) 0.2835(4) 0.091(3) Uani 1 1 d . . . H68A H 0.0236 0.2457 0.3013 0.137 Uiso 1 1 calc R . . H68B H 0.0770 0.2084 0.2396 0.137 Uiso 1 1 calc R . . H68C H 0.1709 0.2308 0.2787 0.137 Uiso 1 1 calc R . . C69 C 0.2022(7) 0.1398(5) 0.4254(4) 0.089(3) Uani 1 1 d . . . H69A H 0.2601 0.1747 0.3905 0.134 Uiso 1 1 calc R . . H69B H 0.2467 0.1013 0.4636 0.134 Uiso 1 1 calc R . . H69C H 0.1337 0.1809 0.4403 0.134 Uiso 1 1 calc R . . C70 C 0.4742(6) -0.0959(5) 0.1518(3) 0.0478(18) Uani 1 1 d . . . C71 C 0.5434(7) -0.1674(5) 0.1312(4) 0.071(2) Uani 1 1 d . . . H71 H 0.5225 -0.2259 0.1536 0.086 Uiso 1 1 calc . . . C72 C 0.6423(8) -0.1563(6) 0.0791(5) 0.088(3) Uani 1 1 d . . . H72 H 0.6880 -0.2070 0.0675 0.106 Uiso 1 1 calc . . . C73 C 0.6736(8) -0.0704(7) 0.0439(4) 0.078(3) Uani 1 1 d . . . H73 H 0.7403 -0.0618 0.0083 0.094 Uiso 1 1 calc . . . C74 C 0.6047(8) 0.0013(5) 0.0623(4) 0.079(3) Uani 1 1 d . . . H74 H 0.6241 0.0600 0.0385 0.094 Uiso 1 1 calc . . . C75 C 0.5069(7) -0.0099(5) 0.1153(4) 0.066(2) Uani 1 1 d . . . H75 H 0.4620 0.0411 0.1267 0.079 Uiso 1 1 calc . . . C80 C 0.2137(8) -0.1543(7) 0.1972(5) 0.074(2) Uani 1 1 d . . . C81 C 0.1840(10) -0.2427(9) 0.2252(4) 0.123(4) Uani 1 1 d . . . H81 H 0.2307 -0.2872 0.2582 0.148 Uiso 1 1 calc . . . C82 C 0.0804(14) -0.2644(12) 0.2024(7) 0.151(7) Uani 1 1 d . . . H82 H 0.0598 -0.3234 0.2205 0.181 Uiso 1 1 calc . . . C83 C 0.0152(16) -0.2022(16) 0.1567(11) 0.182(11) Uani 1 1 d . . . H83 H -0.0538 -0.2179 0.1446 0.219 Uiso 1 1 calc . . . C84 C 0.0419(16) -0.1143(12) 0.1249(10) 0.187(8) Uani 1 1 d . . . H84 H -0.0030 -0.0719 0.0902 0.225 Uiso 1 1 calc . . . C85 C 0.1410(11) -0.0936(7) 0.1486(6) 0.128(4) Uani 1 1 d . . . H85 H 0.1590 -0.0338 0.1300 0.153 Uiso 1 1 calc . . . C90 C 0.5931(7) -0.2460(4) 0.3772(4) 0.055(2) Uani 1 1 d . . . C91 C 0.6833(10) -0.2714(6) 0.3292(5) 0.093(3) Uani 1 1 d . . . H91 H 0.6599 -0.2699 0.2881 0.111 Uiso 1 1 calc . . . C92 C 0.8103(12) -0.2995(8) 0.3421(8) 0.125(5) Uani 1 1 d . . . H92 H 0.8706 -0.3168 0.3093 0.150 Uiso 1 1 calc . . . C93 C 0.8473(13) -0.3021(8) 0.4002(10) 0.135(7) Uani 1 1 d . . . H93 H 0.9318 -0.3234 0.4085 0.162 Uiso 1 1 calc . . . C94 C 0.7618(12) -0.2737(7) 0.4470(6) 0.115(4) Uani 1 1 d . . . H94 H 0.7881 -0.2713 0.4863 0.138 Uiso 1 1 calc . . . C95 C 0.6338(8) -0.2480(5) 0.4362(5) 0.087(3) Uani 1 1 d . . . H95 H 0.5746 -0.2318 0.4699 0.104 Uiso 1 1 calc . . . C100 C 0.3408(7) -0.3075(5) 0.4250(4) 0.058(2) Uani 1 1 d . . . C101 C 0.3160(10) -0.3172(6) 0.4945(5) 0.127(4) Uani 1 1 d . . . H101 H 0.3321 -0.2723 0.5102 0.152 Uiso 1 1 calc . . . C102 C 0.2666(13) -0.3951(9) 0.5412(5) 0.164(5) Uani 1 1 d . . . H102 H 0.2494 -0.4017 0.5877 0.197 Uiso 1 1 calc . . . C103 C 0.2442(14) -0.4604(8) 0.5176(7) 0.159(6) Uani 1 1 d . . . H103 H 0.2201 -0.5147 0.5487 0.190 Uiso 1 1 calc . . . C104 C 0.2560(14) -0.4479(9) 0.4530(7) 0.170(6) Uani 1 1 d . . . H104 H 0.2303 -0.4892 0.4370 0.204 Uiso 1 1 calc . . . C105 C 0.3080(10) -0.3718(6) 0.4067(4) 0.121(4) Uani 1 1 d . . . H105 H 0.3202 -0.3660 0.3603 0.146 Uiso 1 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti11 0.0366(8) 0.0396(8) 0.0474(9) -0.0101(7) -0.0077(7) -0.0081(6) Si11 0.0473(13) 0.0450(13) 0.0463(14) -0.0119(11) -0.0093(11) -0.0056(10) Si12 0.0508(14) 0.0443(13) 0.0589(16) -0.0186(12) -0.0110(12) -0.0025(11) O11 0.042(3) 0.044(3) 0.040(3) -0.009(2) -0.008(2) -0.005(2) O12 0.050(3) 0.044(3) 0.043(3) -0.013(2) -0.006(2) -0.004(2) O13 0.055(3) 0.044(3) 0.052(3) -0.017(2) -0.011(2) -0.001(2) Ti21 0.0328(7) 0.0445(8) 0.0397(8) -0.0111(7) -0.0007(6) -0.0072(6) Si21 0.0596(14) 0.0586(14) 0.0425(14) -0.0213(12) 0.0016(11) -0.0146(11) Si22 0.0561(14) 0.0446(13) 0.0430(14) -0.0109(11) 0.0042(11) -0.0102(11) O21 0.044(3) 0.043(3) 0.034(3) -0.012(2) -0.004(2) -0.002(2) O22 0.046(3) 0.056(3) 0.041(3) -0.019(2) -0.012(2) 0.005(2) O23 0.081(4) 0.046(3) 0.037(3) -0.012(2) 0.002(3) -0.010(3) O1 0.041(3) 0.045(3) 0.053(3) -0.005(2) -0.006(2) -0.011(2) C10 0.041(4) 0.051(5) 0.055(5) 0.001(4) -0.024(4) -0.008(4) C11 0.030(4) 0.035(4) 0.061(5) -0.002(4) -0.014(4) -0.006(3) C12 0.025(4) 0.044(5) 0.055(5) -0.004(4) -0.005(4) -0.001(3) C13 0.037(4) 0.048(5) 0.071(6) -0.011(5) -0.015(4) -0.009(4) C14 0.045(5) 0.052(5) 0.068(6) -0.021(5) -0.023(4) -0.005(4) C15 0.083(6) 0.070(5) 0.064(6) -0.004(5) -0.038(5) -0.011(5) C16 0.063(5) 0.043(5) 0.091(6) -0.010(4) -0.017(5) -0.008(4) C17 0.041(5) 0.072(5) 0.070(6) -0.002(5) 0.006(4) -0.016(4) C18 0.057(5) 0.046(5) 0.117(7) -0.004(5) -0.030(5) -0.015(4) C19 0.118(7) 0.074(6) 0.095(7) -0.032(5) -0.054(6) -0.010(5) C20 0.056(5) 0.054(5) 0.045(5) -0.022(4) -0.014(4) -0.002(4) C21 0.064(6) 0.075(6) 0.053(5) -0.019(5) -0.010(4) -0.011(5) C22 0.061(6) 0.105(7) 0.091(7) -0.036(6) -0.016(5) -0.026(5) C23 0.055(6) 0.137(9) 0.087(8) -0.036(7) -0.027(5) -0.015(6) C24 0.072(7) 0.105(8) 0.104(8) -0.005(6) -0.042(6) 0.002(6) C25 0.082(6) 0.065(6) 0.088(7) -0.008(5) -0.033(6) -0.014(5) C30 0.053(5) 0.043(5) 0.044(5) -0.008(4) -0.003(4) -0.005(4) C31 0.078(6) 0.053(5) 0.051(5) -0.010(4) -0.003(5) -0.015(4) C32 0.079(6) 0.087(7) 0.064(6) -0.036(5) 0.014(5) -0.014(5) C33 0.064(6) 0.080(7) 0.071(6) -0.016(5) 0.009(5) -0.016(5) C34 0.067(6) 0.055(5) 0.076(7) -0.010(5) -0.002(5) -0.018(4) C35 0.064(5) 0.053(5) 0.050(5) -0.014(4) 0.005(4) -0.014(4) C40 0.065(6) 0.039(4) 0.065(6) -0.019(4) -0.008(5) -0.005(4) C41 0.059(6) 0.089(7) 0.072(7) -0.005(5) -0.004(5) -0.014(5) C42 0.048(6) 0.113(8) 0.111(9) -0.003(7) -0.008(6) -0.006(5) C43 0.067(8) 0.100(8) 0.133(11) -0.024(8) 0.013(8) 0.023(6) C44 0.072(8) 0.170(11) 0.141(11) -0.066(9) 0.008(8) 0.023(8) C45 0.078(7) 0.123(8) 0.099(8) -0.052(7) -0.005(6) 0.004(6) C50 0.064(5) 0.032(4) 0.065(6) -0.020(4) -0.020(5) 0.000(4) C51 0.067(6) 0.044(5) 0.071(6) -0.017(5) -0.021(5) -0.005(4) C52 0.087(7) 0.059(6) 0.088(7) -0.010(5) -0.019(6) -0.028(5) C53 0.096(7) 0.061(6) 0.122(9) -0.033(7) -0.045(7) -0.008(5) C54 0.103(8) 0.079(7) 0.085(7) -0.035(6) -0.041(6) -0.009(6) C55 0.079(6) 0.072(6) 0.082(7) -0.035(5) -0.013(5) -0.011(5) C60 0.036(4) 0.071(6) 0.041(5) -0.012(5) 0.003(4) 0.001(4) C61 0.028(4) 0.057(5) 0.068(6) -0.019(5) 0.008(4) -0.016(4) C62 0.037(4) 0.056(5) 0.047(5) -0.019(4) -0.001(4) -0.002(4) C63 0.036(4) 0.058(6) 0.058(6) -0.011(5) 0.007(4) -0.004(4) C64 0.051(5) 0.056(5) 0.058(6) -0.026(5) 0.012(4) -0.008(4) C65 0.082(6) 0.096(6) 0.047(5) -0.022(5) 0.008(5) -0.014(5) C66 0.061(5) 0.082(6) 0.097(7) -0.031(5) 0.004(5) -0.029(5) C67 0.050(5) 0.123(7) 0.098(7) -0.038(6) -0.033(5) -0.005(5) C68 0.080(6) 0.058(6) 0.114(8) -0.015(6) 0.004(5) 0.003(5) C69 0.103(7) 0.105(7) 0.089(7) -0.065(6) 0.000(5) -0.029(6) C70 0.067(5) 0.043(4) 0.036(5) -0.015(4) -0.012(4) -0.005(4) C71 0.079(6) 0.067(6) 0.069(6) -0.032(5) 0.027(5) -0.027(5) C72 0.084(7) 0.076(6) 0.103(8) -0.049(6) 0.027(6) -0.008(5) C73 0.072(6) 0.102(8) 0.061(6) -0.033(6) 0.018(5) -0.023(6) C74 0.080(7) 0.066(6) 0.076(7) -0.009(5) 0.012(5) -0.024(5) C75 0.079(6) 0.063(6) 0.055(5) -0.024(5) -0.004(5) -0.001(5) C80 0.065(6) 0.104(7) 0.074(7) -0.053(6) 0.006(5) -0.027(6) C81 0.151(10) 0.203(12) 0.057(7) -0.062(7) 0.024(6) -0.114(9) C82 0.146(13) 0.265(19) 0.106(11) -0.106(12) 0.056(8) -0.155(14) C83 0.088(11) 0.34(3) 0.19(2) -0.17(3) 0.001(11) -0.046(17) C84 0.139(15) 0.25(2) 0.25(2) -0.171(19) -0.091(14) 0.033(13) C85 0.119(10) 0.142(10) 0.169(12) -0.100(9) -0.072(8) 0.012(8) C90 0.055(5) 0.031(4) 0.067(6) 0.004(4) -0.011(5) -0.009(4) C91 0.076(7) 0.070(6) 0.122(8) -0.040(6) 0.028(7) -0.009(5) C92 0.068(9) 0.067(7) 0.206(16) -0.027(9) 0.037(9) -0.012(7) C93 0.069(9) 0.057(7) 0.27(2) -0.033(11) -0.037(12) -0.009(6) C94 0.103(9) 0.067(7) 0.178(13) -0.023(7) -0.064(9) -0.011(7) C95 0.071(7) 0.063(6) 0.124(9) -0.021(6) -0.031(6) -0.005(5) C100 0.065(5) 0.051(5) 0.053(5) -0.011(4) 0.009(4) -0.022(4) C101 0.197(12) 0.111(8) 0.080(8) -0.019(7) 0.010(8) -0.086(8) C102 0.261(15) 0.141(11) 0.077(8) 0.000(8) 0.037(9) -0.112(11) C103 0.237(15) 0.084(8) 0.152(13) -0.034(9) 0.057(12) -0.094(9) C104 0.286(17) 0.138(11) 0.122(11) -0.070(10) 0.060(12) -0.137(11) C105 0.205(11) 0.096(8) 0.080(7) -0.033(6) 0.043(7) -0.105(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti11 O1 1.827(4) . ? Ti11 O11 1.849(4) . ? Ti11 O12 1.874(4) . ? Ti11 C10 2.354(6) . ? Ti11 C11 2.354(6) . ? Ti11 C14 2.371(6) . ? Ti11 C12 2.382(6) . ? Ti11 C13 2.383(6) . ? Si11 O11 1.620(4) . ? Si11 O13 1.640(4) . ? Si11 C30 1.853(7) . ? Si11 C20 1.856(7) . ? Si12 O13 1.622(4) . ? Si12 O12 1.627(4) . ? Si12 C50 1.848(7) . ? Si12 C40 1.858(7) . ? Ti21 O1 1.806(4) . ? Ti21 O22 1.847(4) . ? Ti21 O21 1.855(4) . ? Ti21 C63 2.347(7) . ? Ti21 C61 2.356(6) . ? Ti21 C60 2.361(7) . ? Ti21 C62 2.362(6) . ? Ti21 C64 2.379(7) . ? Si21 O22 1.618(4) . ? Si21 O23 1.634(4) . ? Si21 C70 1.841(7) . ? Si21 C80 1.849(8) . ? Si22 O21 1.626(4) . ? Si22 O23 1.644(4) . ? Si22 C100 1.845(7) . ? Si22 C90 1.856(7) . ? C10 C11 1.396(8) . ? C10 C14 1.418(8) . ? C10 C15 1.502(8) . ? C11 C12 1.407(8) . ? C11 C16 1.528(8) . ? C12 C13 1.410(8) . ? C12 C17 1.482(8) . ? C13 C14 1.414(9) . ? C13 C18 1.517(8) . ? C14 C19 1.492(9) . ? C20 C21 1.369(8) . ? C20 C25 1.395(9) . ? C21 C22 1.383(9) . ? C22 C23 1.358(10) . ? C23 C24 1.359(11) . ? C24 C25 1.382(10) . ? C30 C31 1.373(8) . ? C30 C35 1.390(9) . ? C31 C32 1.374(9) . ? C32 C33 1.372(10) . ? C33 C34 1.358(10) . ? C34 C35 1.381(9) . ? C40 C41 1.376(9) . ? C40 C45 1.379(10) . ? C41 C42 1.389(10) . ? C42 C43 1.379(12) . ? C43 C44 1.329(12) . ? C44 C45 1.374(11) . ? C50 C55 1.394(9) . ? C50 C51 1.396(9) . ? C51 C52 1.368(9) . ? C52 C53 1.354(11) . ? C53 C54 1.340(10) . ? C54 C55 1.406(10) . ? C60 C61 1.389(9) . ? C60 C64 1.411(8) . ? C60 C65 1.509(8) . ? C61 C62 1.403(8) . ? C61 C66 1.511(8) . ? C62 C63 1.395(8) . ? C62 C67 1.506(9) . ? C63 C64 1.395(9) . ? C63 C68 1.522(8) . ? C64 C69 1.511(9) . ? C70 C71 1.371(8) . ? C70 C75 1.386(8) . ? C71 C72 1.372(9) . ? C72 C73 1.374(10) . ? C73 C74 1.352(9) . ? C74 C75 1.375(9) . ? C80 C85 1.366(11) . ? C80 C81 1.388(11) . ? C81 C82 1.432(13) . ? C82 C83 1.30(2) . ? C83 C84 1.37(2) . ? C84 C85 1.393(16) . ? C90 C95 1.371(10) . ? C90 C91 1.371(10) . ? C91 C92 1.396(13) . ? C92 C93 1.330(16) . ? C93 C94 1.347(16) . ? C94 C95 1.393(11) . ? C100 C105 1.324(9) . ? C100 C101 1.389(10) . ? C101 C102 1.410(12) . ? C102 C103 1.360(14) . ? C103 C104 1.283(14) . ? C104 C105 1.400(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti11 O11 105.54(18) . . ? O1 Ti11 O12 107.23(18) . . ? O11 Ti11 O12 97.96(17) . . ? O1 Ti11 C10 85.2(2) . . ? O11 Ti11 C10 140.5(2) . . ? O12 Ti11 C10 115.3(2) . . ? O1 Ti11 C11 91.2(2) . . ? O11 Ti11 C11 106.3(2) . . ? O12 Ti11 C11 144.3(2) . . ? C10 Ti11 C11 34.5(2) . . ? O1 Ti11 C14 113.9(2) . . ? O11 Ti11 C14 136.7(2) . . ? O12 Ti11 C14 87.1(2) . . ? C10 Ti11 C14 34.9(2) . . ? C11 Ti11 C14 57.3(2) . . ? O1 Ti11 C12 124.0(2) . . ? O11 Ti11 C12 86.1(2) . . ? O12 Ti11 C12 125.5(2) . . ? C10 Ti11 C12 57.8(2) . . ? C11 Ti11 C12 34.56(19) . . ? C14 Ti11 C12 57.6(2) . . ? O1 Ti11 C13 142.8(2) . . ? O11 Ti11 C13 102.1(2) . . ? O12 Ti11 C13 92.8(2) . . ? C10 Ti11 C13 57.8(2) . . ? C11 Ti11 C13 57.1(2) . . ? C14 Ti11 C13 34.6(2) . . ? C12 Ti11 C13 34.4(2) . . ? O11 Si11 O13 108.1(2) . . ? O11 Si11 C30 110.6(3) . . ? O13 Si11 C30 108.9(3) . . ? O11 Si11 C20 108.6(3) . . ? O13 Si11 C20 111.0(3) . . ? C30 Si11 C20 109.6(3) . . ? O13 Si12 O12 109.2(2) . . ? O13 Si12 C50 108.5(3) . . ? O12 Si12 C50 109.9(3) . . ? O13 Si12 C40 108.2(3) . . ? O12 Si12 C40 110.6(3) . . ? C50 Si12 C40 110.4(3) . . ? Si11 O11 Ti11 134.7(2) . . ? Si12 O12 Ti11 132.9(2) . . ? Si12 O13 Si11 134.9(3) . . ? O1 Ti21 O22 104.21(19) . . ? O1 Ti21 O21 108.69(18) . . ? O22 Ti21 O21 97.66(17) . . ? O1 Ti21 C63 89.8(2) . . ? O22 Ti21 C63 108.5(2) . . ? O21 Ti21 C63 143.2(2) . . ? O1 Ti21 C61 143.0(2) . . ? O22 Ti21 C61 102.4(2) . . ? O21 Ti21 C61 92.6(2) . . ? C63 Ti21 C61 57.3(2) . . ? O1 Ti21 C60 115.6(2) . . ? O22 Ti21 C60 136.6(2) . . ? O21 Ti21 C60 85.9(2) . . ? C63 Ti21 C60 57.3(2) . . ? C61 Ti21 C60 34.2(2) . . ? O1 Ti21 C62 122.1(2) . . ? O22 Ti21 C62 87.6(2) . . ? O21 Ti21 C62 125.9(2) . . ? C63 Ti21 C62 34.5(2) . . ? C61 Ti21 C62 34.6(2) . . ? C60 Ti21 C62 57.3(2) . . ? O1 Ti21 C64 86.2(2) . . ? O22 Ti21 C64 142.3(2) . . ? O21 Ti21 C64 113.4(2) . . ? C63 Ti21 C64 34.3(2) . . ? C61 Ti21 C64 57.2(2) . . ? C60 Ti21 C64 34.6(2) . . ? C62 Ti21 C64 57.2(2) . . ? O22 Si21 O23 109.6(2) . . ? O22 Si21 C70 111.3(3) . . ? O23 Si21 C70 108.0(3) . . ? O22 Si21 C80 109.7(3) . . ? O23 Si21 C80 108.1(4) . . ? C70 Si21 C80 110.0(3) . . ? O21 Si22 O23 109.0(2) . . ? O21 Si22 C100 113.9(3) . . ? O23 Si22 C100 107.1(3) . . ? O21 Si22 C90 110.6(3) . . ? O23 Si22 C90 109.9(3) . . ? C100 Si22 C90 106.2(3) . . ? Si22 O21 Ti21 135.0(2) . . ? Si21 O22 Ti21 135.1(2) . . ? Si21 O23 Si22 133.4(3) . . ? Ti21 O1 Ti11 161.6(3) . . ? C11 C10 C14 107.3(6) . . ? C11 C10 C15 126.1(7) . . ? C14 C10 C15 126.6(7) . . ? C11 C10 Ti11 72.8(4) . . ? C14 C10 Ti11 73.2(4) . . ? C15 C10 Ti11 121.5(4) . . ? C10 C11 C12 109.6(6) . . ? C10 C11 C16 125.8(6) . . ? C12 C11 C16 124.6(7) . . ? C10 C11 Ti11 72.7(4) . . ? C12 C11 Ti11 73.8(3) . . ? C16 C11 Ti11 121.6(4) . . ? C11 C12 C13 107.1(7) . . ? C11 C12 C17 126.1(7) . . ? C13 C12 C17 126.6(7) . . ? C11 C12 Ti11 71.7(4) . . ? C13 C12 Ti11 72.8(4) . . ? C17 C12 Ti11 123.9(4) . . ? C12 C13 C14 108.2(6) . . ? C12 C13 C18 125.8(7) . . ? C14 C13 C18 125.8(7) . . ? C12 C13 Ti11 72.7(4) . . ? C14 C13 Ti11 72.2(4) . . ? C18 C13 Ti11 125.0(4) . . ? C13 C14 C10 107.9(7) . . ? C13 C14 C19 126.1(7) . . ? C10 C14 C19 126.0(7) . . ? C13 C14 Ti11 73.2(4) . . ? C10 C14 Ti11 71.9(4) . . ? C19 C14 Ti11 121.7(5) . . ? C21 C20 C25 116.7(7) . . ? C21 C20 Si11 123.7(6) . . ? C25 C20 Si11 119.6(6) . . ? C20 C21 C22 122.4(7) . . ? C23 C22 C21 119.7(8) . . ? C22 C23 C24 119.6(8) . . ? C23 C24 C25 120.9(8) . . ? C24 C25 C20 120.6(7) . . ? C31 C30 C35 117.5(7) . . ? C31 C30 Si11 119.8(6) . . ? C35 C30 Si11 122.3(6) . . ? C30 C31 C32 122.2(7) . . ? C33 C32 C31 119.3(7) . . ? C34 C33 C32 120.0(8) . . ? C33 C34 C35 120.7(8) . . ? C34 C35 C30 120.3(7) . . ? C41 C40 C45 117.7(8) . . ? C41 C40 Si12 122.7(7) . . ? C45 C40 Si12 119.6(7) . . ? C40 C41 C42 120.6(8) . . ? C43 C42 C41 119.1(9) . . ? C44 C43 C42 120.8(10) . . ? C43 C44 C45 120.1(11) . . ? C44 C45 C40 121.6(9) . . ? C55 C50 C51 115.9(7) . . ? C55 C50 Si12 121.6(6) . . ? C51 C50 Si12 122.4(6) . . ? C52 C51 C50 121.3(7) . . ? C53 C52 C51 120.4(8) . . ? C54 C53 C52 122.2(9) . . ? C53 C54 C55 117.8(8) . . ? C50 C55 C54 122.4(8) . . ? C61 C60 C64 108.2(6) . . ? C61 C60 C65 125.8(7) . . ? C64 C60 C65 125.9(8) . . ? C61 C60 Ti21 72.7(4) . . ? C64 C60 Ti21 73.4(4) . . ? C65 C60 Ti21 121.7(4) . . ? C60 C61 C62 108.3(6) . . ? C60 C61 C66 127.7(7) . . ? C62 C61 C66 124.0(7) . . ? C60 C61 Ti21 73.1(4) . . ? C62 C61 Ti21 72.9(4) . . ? C66 C61 Ti21 121.2(5) . . ? C63 C62 C61 107.4(7) . . ? C63 C62 C67 126.0(7) . . ? C61 C62 C67 126.6(7) . . ? C63 C62 Ti21 72.2(4) . . ? C61 C62 Ti21 72.5(4) . . ? C67 C62 Ti21 121.2(4) . . ? C62 C63 C64 109.0(7) . . ? C62 C63 C68 126.1(7) . . ? C64 C63 C68 124.7(8) . . ? C62 C63 Ti21 73.4(4) . . ? C64 C63 Ti21 74.1(4) . . ? C68 C63 Ti21 123.1(4) . . ? C63 C64 C60 107.1(7) . . ? C63 C64 C69 125.6(7) . . ? C60 C64 C69 127.3(8) . . ? C63 C64 Ti21 71.6(4) . . ? C60 C64 Ti21 72.0(4) . . ? C69 C64 Ti21 121.3(5) . . ? C71 C70 C75 116.1(7) . . ? C71 C70 Si21 119.3(6) . . ? C75 C70 Si21 124.5(6) . . ? C70 C71 C72 122.9(7) . . ? C71 C72 C73 120.0(7) . . ? C74 C73 C72 118.1(8) . . ? C73 C74 C75 122.0(8) . . ? C74 C75 C70 121.0(7) . . ? C85 C80 C81 116.7(9) . . ? C85 C80 Si21 120.7(8) . . ? C81 C80 Si21 122.6(8) . . ? C80 C81 C82 118.9(11) . . ? C83 C82 C81 120.4(18) . . ? C82 C83 C84 124(2) . . ? C83 C84 C85 115(2) . . ? C80 C85 C84 124.9(13) . . ? C95 C90 C91 117.3(8) . . ? C95 C90 Si22 120.0(7) . . ? C91 C90 Si22 122.7(8) . . ? C90 C91 C92 120.0(10) . . ? C93 C92 C91 121.7(15) . . ? C92 C93 C94 119.7(15) . . ? C93 C94 C95 119.7(13) . . ? C90 C95 C94 121.6(9) . . ? C105 C100 C101 115.8(7) . . ? C105 C100 Si22 124.4(7) . . ? C101 C100 Si22 119.7(7) . . ? C100 C101 C102 119.9(9) . . ? C103 C102 C101 119.5(11) . . ? C104 C103 C102 120.7(12) . . ? C103 C104 C105 119.5(11) . . ? C100 C105 C104 124.0(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.304 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.067 data_4 _database_code_depnum_ccdc_archive 'CCDC 626324' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H50 Cl2 O4 Si2 Ti2, C2 H5 O0.5' _chemical_formula_sum 'C46 H55 Cl2 O4.5 Si2 Ti2' _chemical_formula_weight 902.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.959(3) _cell_length_b 18.851(5) _cell_length_c 23.007(6) _cell_angle_alpha 82.568(5) _cell_angle_beta 80.411(5) _cell_angle_gamma 82.677(5) _cell_volume 4620(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7732 _exptl_absorpt_correction_T_max 0.9456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30563 _diffrn_reflns_av_R_equivalents 0.0997 _diffrn_reflns_av_sigmaI/netI 0.2045 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15982 _reflns_number_gt 7154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15982 _refine_ls_number_parameters 1040 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1799 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1337 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.41700(11) 0.19089(6) 0.84666(5) 0.0286(3) Uani 1 1 d . . . Ti2 Ti 0.34365(11) 0.25617(6) 0.98466(5) 0.0277(3) Uani 1 1 d . . . Ti3 Ti 0.83754(11) 0.70066(6) 0.56610(5) 0.0304(3) Uani 1 1 d . . . Ti4 Ti 0.54416(11) 0.79595(6) 0.55367(5) 0.0292(3) Uani 1 1 d . . . Si1 Si 0.05090(16) 0.28742(9) 0.94963(7) 0.0271(5) Uani 1 1 d . . . Si2 Si 0.15550(17) 0.29959(9) 0.81477(8) 0.0290(5) Uani 1 1 d . . . Si3 Si 0.47847(17) 0.73445(9) 0.69959(7) 0.0276(5) Uani 1 1 d . . . Si4 Si 0.67610(17) 0.60139(9) 0.68024(7) 0.0267(4) Uani 1 1 d . . . Cl1 Cl 0.36160(18) 0.07556(8) 0.86361(8) 0.0486(5) Uani 1 1 d . . . Cl2 Cl 0.42747(17) 0.36388(8) 0.96639(7) 0.0417(5) Uani 1 1 d . . . Cl3 Cl 0.93490(17) 0.78342(9) 0.60038(8) 0.0460(5) Uani 1 1 d . . . Cl4 Cl 0.45137(17) 0.72816(8) 0.50164(7) 0.0433(5) Uani 1 1 d . . . O1 O 0.4184(4) 0.2113(2) 0.92061(16) 0.0303(11) Uani 1 1 d . . . O2 O 0.1837(4) 0.2809(2) 0.97285(16) 0.0297(11) Uani 1 1 d . . . O3 O 0.0692(4) 0.3105(2) 0.87875(16) 0.0313(11) Uani 1 1 d . . . O4 O 0.2780(4) 0.24216(19) 0.82353(16) 0.0301(11) Uani 1 1 d . . . O5 O 0.7051(4) 0.75698(19) 0.54118(16) 0.0323(11) Uani 1 1 d . . . O6 O 0.4860(4) 0.76693(19) 0.63023(15) 0.0306(11) Uani 1 1 d . . . O7 O 0.5563(4) 0.65589(19) 0.70459(16) 0.0324(11) Uani 1 1 d . . . O8 O 0.7739(4) 0.6468(2) 0.63306(16) 0.0304(11) Uani 1 1 d . . . C1 C 0.6270(6) 0.2161(3) 0.8301(3) 0.0346(17) Uani 1 1 d . . . C2 C 0.6297(6) 0.1466(3) 0.8146(3) 0.0374(18) Uani 1 1 d . . . C3 C 0.5635(6) 0.1528(3) 0.7652(3) 0.0313(17) Uani 1 1 d . . . C4 C 0.5227(6) 0.2252(3) 0.7511(3) 0.0317(17) Uani 1 1 d . . . C5 C 0.5590(6) 0.2648(3) 0.7918(3) 0.0294(16) Uani 1 1 d . . . C6 C 0.6910(6) 0.2380(4) 0.8769(3) 0.0441(19) Uani 1 1 d . . . H6A H 0.7170 0.1953 0.9028 0.066 Uiso 1 1 calc R . . H6B H 0.6334 0.2714 0.9005 0.066 Uiso 1 1 calc R . . H6C H 0.7643 0.2618 0.8579 0.066 Uiso 1 1 calc R . . C7 C 0.6952(7) 0.0797(4) 0.8429(3) 0.053(2) Uani 1 1 d . . . H7A H 0.7675 0.0626 0.8151 0.079 Uiso 1 1 calc R . . H7B H 0.6380 0.0425 0.8532 0.079 Uiso 1 1 calc R . . H7C H 0.7228 0.0902 0.8789 0.079 Uiso 1 1 calc R . . C8 C 0.5509(7) 0.0907(3) 0.7325(3) 0.053(2) Uani 1 1 d . . . H8A H 0.4719 0.0991 0.7167 0.080 Uiso 1 1 calc R . . H8B H 0.5523 0.0462 0.7598 0.080 Uiso 1 1 calc R . . H8C H 0.6201 0.0863 0.6998 0.080 Uiso 1 1 calc R . . C9 C 0.4532(6) 0.2552(3) 0.6996(3) 0.0393(18) Uani 1 1 d . . . H9A H 0.4263 0.3065 0.7020 0.059 Uiso 1 1 calc R . . H9B H 0.3802 0.2293 0.7016 0.059 Uiso 1 1 calc R . . H9C H 0.5084 0.2491 0.6620 0.059 Uiso 1 1 calc R . . C10 C 0.5394(7) 0.3448(3) 0.7927(3) 0.048(2) Uani 1 1 d . . . H10A H 0.6202 0.3640 0.7855 0.072 Uiso 1 1 calc R . . H10B H 0.4946 0.3562 0.8315 0.072 Uiso 1 1 calc R . . H10C H 0.4904 0.3666 0.7617 0.072 Uiso 1 1 calc R . . C11 C 0.4661(6) 0.2210(3) 1.0618(3) 0.0327(17) Uani 1 1 d . . . C12 C 0.3507(6) 0.2552(3) 1.0872(3) 0.0335(17) Uani 1 1 d . . . C13 C 0.2569(6) 0.2123(3) 1.0826(3) 0.0355(17) Uani 1 1 d . . . C14 C 0.3149(6) 0.1534(3) 1.0510(3) 0.0300(16) Uani 1 1 d . . . C15 C 0.4450(6) 0.1577(3) 1.0399(3) 0.0264(16) Uani 1 1 d . . . C16 C 0.5905(6) 0.2468(3) 1.0611(3) 0.0437(19) Uani 1 1 d . . . H16A H 0.6289 0.2211 1.0945 0.066 Uiso 1 1 calc R . . H16B H 0.5794 0.2986 1.0646 0.066 Uiso 1 1 calc R . . H16C H 0.6444 0.2375 1.0238 0.066 Uiso 1 1 calc R . . C17 C 0.3302(7) 0.3235(3) 1.1175(3) 0.050(2) Uani 1 1 d . . . H17A H 0.2477 0.3484 1.1129 0.076 Uiso 1 1 calc R . . H17B H 0.3941 0.3550 1.0994 0.076 Uiso 1 1 calc R . . H17C H 0.3357 0.3113 1.1597 0.076 Uiso 1 1 calc R . . C18 C 0.1220(6) 0.2252(4) 1.1055(3) 0.050(2) Uani 1 1 d . . . H18A H 0.1073 0.2087 1.1480 0.075 Uiso 1 1 calc R . . H18B H 0.0752 0.1988 1.0843 0.075 Uiso 1 1 calc R . . H18C H 0.0945 0.2768 1.0992 0.075 Uiso 1 1 calc R . . C19 C 0.2513(6) 0.0935(3) 1.0371(3) 0.0412(19) Uani 1 1 d . . . H19A H 0.2593 0.0525 1.0675 0.062 Uiso 1 1 calc R . . H19B H 0.2899 0.0790 0.9982 0.062 Uiso 1 1 calc R . . H19C H 0.1630 0.1099 1.0363 0.062 Uiso 1 1 calc R . . C20 C 0.5393(6) 0.1038(3) 1.0124(3) 0.0397(19) Uani 1 1 d . . . H20A H 0.6185 0.1245 1.0003 0.060 Uiso 1 1 calc R . . H20B H 0.5114 0.0899 0.9776 0.060 Uiso 1 1 calc R . . H20C H 0.5505 0.0613 1.0412 0.060 Uiso 1 1 calc R . . C21 C -0.0158(6) 0.1998(3) 0.9648(3) 0.0318(17) Uani 1 1 d . . . C22 C -0.0946(6) 0.1824(3) 1.0166(3) 0.0377(18) Uani 1 1 d . . . H22 H -0.1177 0.2165 1.0445 0.045 Uiso 1 1 calc R . . C23 C -0.1408(7) 0.1158(4) 1.0287(3) 0.050(2) Uani 1 1 d . . . H23 H -0.1941 0.1045 1.0648 0.060 Uiso 1 1 calc R . . C24 C -0.1093(8) 0.0669(4) 0.9885(4) 0.060(2) Uani 1 1 d . . . H24 H -0.1403 0.0213 0.9967 0.072 Uiso 1 1 calc R . . C25 C -0.0330(9) 0.0836(4) 0.9364(4) 0.062(3) Uani 1 1 d . . . H25 H -0.0131 0.0500 0.9080 0.075 Uiso 1 1 calc R . . C26 C 0.0146(7) 0.1481(4) 0.9250(3) 0.045(2) Uani 1 1 d . . . H26 H 0.0697 0.1582 0.8892 0.055 Uiso 1 1 calc R . . C27 C -0.0571(6) 0.3574(3) 0.9874(2) 0.0232(15) Uani 1 1 d . . . C28 C -0.0158(6) 0.3994(3) 1.0243(3) 0.0345(17) Uani 1 1 d . . . H28 H 0.0687 0.3927 1.0305 0.041 Uiso 1 1 calc R . . C29 C -0.0996(7) 0.4512(3) 1.0521(3) 0.0426(19) Uani 1 1 d . . . H29 H -0.0720 0.4789 1.0782 0.051 Uiso 1 1 calc R . . C30 C -0.2211(7) 0.4629(3) 1.0426(3) 0.047(2) Uani 1 1 d . . . H30 H -0.2770 0.4993 1.0608 0.057 Uiso 1 1 calc R . . C31 C -0.2607(7) 0.4213(3) 1.0064(3) 0.0440(19) Uani 1 1 d . . . H31 H -0.3450 0.4286 0.9999 0.053 Uiso 1 1 calc R . . C32 C -0.1799(6) 0.3690(3) 0.9793(3) 0.0387(18) Uani 1 1 d . . . H32 H -0.2095 0.3405 0.9546 0.046 Uiso 1 1 calc R . . C33 C 0.0602(6) 0.2628(3) 0.7687(3) 0.0318(17) Uani 1 1 d . . . C34 C -0.0453(6) 0.3018(4) 0.7512(3) 0.0407(19) Uani 1 1 d . . . H34 H -0.0650 0.3500 0.7605 0.049 Uiso 1 1 calc R . . C35 C -0.1225(7) 0.2746(4) 0.7212(3) 0.052(2) Uani 1 1 d . . . H35 H -0.1931 0.3039 0.7092 0.063 Uiso 1 1 calc R . . C36 C -0.0980(8) 0.2048(5) 0.7086(3) 0.060(2) Uani 1 1 d . . . H36 H -0.1529 0.1851 0.6888 0.072 Uiso 1 1 calc R . . C37 C 0.0054(8) 0.1635(4) 0.7245(3) 0.058(2) Uani 1 1 d . . . H37 H 0.0232 0.1153 0.7152 0.069 Uiso 1 1 calc R . . C38 C 0.0848(7) 0.1922(3) 0.7543(3) 0.0406(19) Uani 1 1 d . . . H38 H 0.1568 0.1632 0.7651 0.049 Uiso 1 1 calc R . . C39 C 0.2023(6) 0.3888(3) 0.7828(3) 0.0293(16) Uani 1 1 d . . . C40 C 0.2419(6) 0.4333(3) 0.8189(3) 0.0360(18) Uani 1 1 d . . . H40 H 0.2410 0.4176 0.8599 0.043 Uiso 1 1 calc R . . C41 C 0.2818(7) 0.4992(4) 0.7964(3) 0.0446(19) Uani 1 1 d . . . H41 H 0.3085 0.5280 0.8219 0.053 Uiso 1 1 calc R . . C42 C 0.2833(7) 0.5233(4) 0.7378(4) 0.054(2) Uani 1 1 d . . . H42 H 0.3104 0.5689 0.7224 0.065 Uiso 1 1 calc R . . C43 C 0.2452(7) 0.4810(4) 0.7011(3) 0.049(2) Uani 1 1 d . . . H43 H 0.2463 0.4975 0.6602 0.059 Uiso 1 1 calc R . . C44 C 0.2053(6) 0.4150(3) 0.7234(3) 0.0388(18) Uani 1 1 d . . . H44 H 0.1791 0.3867 0.6974 0.047 Uiso 1 1 calc R . . C45 C 0.9518(6) 0.5931(3) 0.5367(3) 0.0339(17) Uani 1 1 d . . . C46 C 0.8623(6) 0.6172(4) 0.4979(3) 0.0341(17) Uani 1 1 d . . . C47 C 0.8967(6) 0.6813(4) 0.4642(3) 0.0342(17) Uani 1 1 d . . . C48 C 1.0048(6) 0.6989(4) 0.4836(3) 0.0388(18) Uani 1 1 d . . . C49 C 1.0368(6) 0.6446(4) 0.5276(3) 0.0397(18) Uani 1 1 d . . . C50 C 0.9563(6) 0.5245(3) 0.5793(3) 0.049(2) Uani 1 1 d . . . H50A H 0.8747 0.5062 0.5866 0.074 Uiso 1 1 calc R . . H50B H 0.9778 0.5346 0.6169 0.074 Uiso 1 1 calc R . . H50C H 1.0193 0.4883 0.5619 0.074 Uiso 1 1 calc R . . C51 C 0.7553(6) 0.5786(3) 0.4908(3) 0.046(2) Uani 1 1 d . . . H51A H 0.7684 0.5634 0.4509 0.069 Uiso 1 1 calc R . . H51B H 0.6779 0.6110 0.4965 0.069 Uiso 1 1 calc R . . H51C H 0.7496 0.5363 0.5203 0.069 Uiso 1 1 calc R . . C52 C 0.8305(7) 0.7210(4) 0.4155(3) 0.056(2) Uani 1 1 d . . . H52A H 0.8543 0.7701 0.4068 0.084 Uiso 1 1 calc R . . H52B H 0.7403 0.7228 0.4282 0.084 Uiso 1 1 calc R . . H52C H 0.8537 0.6960 0.3799 0.084 Uiso 1 1 calc R . . C53 C 1.0736(7) 0.7618(4) 0.4585(3) 0.060(2) Uani 1 1 d . . . H53A H 1.1470 0.7462 0.4307 0.090 Uiso 1 1 calc R . . H53B H 1.0998 0.7828 0.4906 0.090 Uiso 1 1 calc R . . H53C H 1.0191 0.7980 0.4375 0.090 Uiso 1 1 calc R . . C54 C 1.1500(6) 0.6390(4) 0.5585(3) 0.051(2) Uani 1 1 d . . . H54A H 1.1314 0.6144 0.5987 0.076 Uiso 1 1 calc R . . H54B H 1.1716 0.6874 0.5608 0.076 Uiso 1 1 calc R . . H54C H 1.2203 0.6115 0.5362 0.076 Uiso 1 1 calc R . . C55 C 0.6221(7) 0.9039(3) 0.5090(3) 0.0349(18) Uani 1 1 d . . . C56 C 0.5280(8) 0.8935(3) 0.4777(3) 0.0395(19) Uani 1 1 d . . . C57 C 0.4146(8) 0.8973(3) 0.5179(3) 0.043(2) Uani 1 1 d . . . C58 C 0.4408(7) 0.9107(3) 0.5739(3) 0.0379(19) Uani 1 1 d . . . C59 C 0.5705(7) 0.9133(3) 0.5680(3) 0.0347(18) Uani 1 1 d . . . C60 C 0.7570(7) 0.9061(3) 0.4834(3) 0.050(2) Uani 1 1 d . . . H60A H 0.7725 0.9560 0.4693 0.075 Uiso 1 1 calc R . . H60B H 0.7780 0.8768 0.4502 0.075 Uiso 1 1 calc R . . H60C H 0.8086 0.8870 0.5140 0.075 Uiso 1 1 calc R . . C61 C 0.5410(8) 0.8834(4) 0.4137(3) 0.063(3) Uani 1 1 d . . . H61A H 0.4793 0.8526 0.4081 0.095 Uiso 1 1 calc R . . H61B H 0.6249 0.8606 0.4005 0.095 Uiso 1 1 calc R . . H61C H 0.5276 0.9303 0.3904 0.095 Uiso 1 1 calc R . . C62 C 0.2873(7) 0.8910(4) 0.5037(3) 0.063(2) Uani 1 1 d . . . H62A H 0.2370 0.8680 0.5386 0.094 Uiso 1 1 calc R . . H62B H 0.2954 0.8618 0.4707 0.094 Uiso 1 1 calc R . . H62C H 0.2467 0.9391 0.4925 0.094 Uiso 1 1 calc R . . C63 C 0.3459(7) 0.9204(3) 0.6279(3) 0.046(2) Uani 1 1 d . . . H63A H 0.3074 0.9703 0.6259 0.069 Uiso 1 1 calc R . . H63B H 0.3864 0.9092 0.6634 0.069 Uiso 1 1 calc R . . H63C H 0.2819 0.8880 0.6299 0.069 Uiso 1 1 calc R . . C64 C 0.6411(6) 0.9273(3) 0.6157(3) 0.0432(19) Uani 1 1 d . . . H64A H 0.7188 0.8950 0.6143 0.065 Uiso 1 1 calc R . . H64B H 0.5901 0.9186 0.6547 0.065 Uiso 1 1 calc R . . H64C H 0.6601 0.9774 0.6092 0.065 Uiso 1 1 calc R . . C65 C 0.3171(6) 0.7239(3) 0.7318(3) 0.0269(16) Uani 1 1 d . . . C66 C 0.2860(7) 0.7027(3) 0.7924(3) 0.0364(17) Uani 1 1 d . . . H66 H 0.3483 0.6981 0.8172 0.044 Uiso 1 1 calc R . . C67 C 0.1663(8) 0.6882(3) 0.8171(3) 0.050(2) Uani 1 1 d . . . H67 H 0.1472 0.6754 0.8586 0.060 Uiso 1 1 calc R . . C68 C 0.0754(7) 0.6922(4) 0.7822(4) 0.056(2) Uani 1 1 d . . . H68 H -0.0056 0.6801 0.7988 0.067 Uiso 1 1 calc R . . C69 C 0.1031(8) 0.7139(4) 0.7233(4) 0.055(2) Uani 1 1 d . . . H69 H 0.0396 0.7187 0.6991 0.066 Uiso 1 1 calc R . . C70 C 0.2207(7) 0.7289(3) 0.6980(3) 0.0367(18) Uani 1 1 d . . . H70 H 0.2372 0.7431 0.6565 0.044 Uiso 1 1 calc R . . C71 C 0.5505(7) 0.7932(3) 0.7410(3) 0.0326(17) Uani 1 1 d . . . C72 C 0.6790(7) 0.7891(4) 0.7352(3) 0.0431(19) Uani 1 1 d . . . H72 H 0.7282 0.7545 0.7121 0.052 Uiso 1 1 calc R . . C73 C 0.7379(8) 0.8342(4) 0.7620(3) 0.057(2) Uani 1 1 d . . . H73 H 0.8261 0.8305 0.7576 0.069 Uiso 1 1 calc R . . C74 C 0.6669(9) 0.8837(4) 0.7947(3) 0.057(2) Uani 1 1 d . . . H74 H 0.7066 0.9150 0.8129 0.068 Uiso 1 1 calc R . . C75 C 0.5384(8) 0.8898(3) 0.8021(3) 0.048(2) Uani 1 1 d . . . H75 H 0.4902 0.9239 0.8260 0.058 Uiso 1 1 calc R . . C76 C 0.4798(7) 0.8446(3) 0.7738(3) 0.045(2) Uani 1 1 d . . . H76 H 0.3916 0.8494 0.7772 0.055 Uiso 1 1 calc R . . C77 C 0.6154(6) 0.5334(3) 0.6437(3) 0.0289(16) Uani 1 1 d . . . C78 C 0.5210(6) 0.5535(3) 0.6088(3) 0.0361(17) Uani 1 1 d . . . H78 H 0.4827 0.6017 0.6059 0.043 Uiso 1 1 calc R . . C79 C 0.4831(6) 0.5039(4) 0.5786(3) 0.0416(19) Uani 1 1 d . . . H79 H 0.4192 0.5188 0.5550 0.050 Uiso 1 1 calc R . . C80 C 0.5350(7) 0.4331(4) 0.5817(3) 0.047(2) Uani 1 1 d . . . H80 H 0.5077 0.3997 0.5604 0.056 Uiso 1 1 calc R . . C81 C 0.6277(7) 0.4119(4) 0.6164(3) 0.048(2) Uani 1 1 d . . . H81 H 0.6644 0.3634 0.6194 0.058 Uiso 1 1 calc R . . C82 C 0.6668(6) 0.4611(3) 0.6467(3) 0.0376(18) Uani 1 1 d . . . H82 H 0.7306 0.4457 0.6704 0.045 Uiso 1 1 calc R . . C83 C 0.7514(6) 0.5579(3) 0.7443(3) 0.0261(16) Uani 1 1 d . . . C84 C 0.6838(7) 0.5191(3) 0.7907(3) 0.0420(19) Uani 1 1 d . . . H84 H 0.5985 0.5158 0.7895 0.050 Uiso 1 1 calc R . . C85 C 0.7364(7) 0.4847(4) 0.8393(3) 0.049(2) Uani 1 1 d . . . H85 H 0.6871 0.4591 0.8711 0.059 Uiso 1 1 calc R . . C86 C 0.8603(8) 0.4880(4) 0.8409(3) 0.054(2) Uani 1 1 d . . . H86 H 0.8976 0.4638 0.8735 0.065 Uiso 1 1 calc R . . C87 C 0.9303(7) 0.5264(4) 0.7953(3) 0.050(2) Uani 1 1 d . . . H87 H 1.0157 0.5294 0.7966 0.060 Uiso 1 1 calc R . . C88 C 0.8758(6) 0.5612(3) 0.7468(3) 0.0379(18) Uani 1 1 d . . . H88 H 0.9248 0.5874 0.7154 0.046 Uiso 1 1 calc R . . O9 O 0.0391(6) 0.9794(3) 0.7047(3) 0.0834(19) Uani 1 1 d . . . C91 C 0.0595(12) 0.9342(6) 0.7556(5) 0.120(4) Uani 1 1 d . . . H91A H 0.0992 0.8869 0.7440 0.144 Uiso 1 1 calc R . . H91B H -0.0219 0.9266 0.7802 0.144 Uiso 1 1 calc R . . C92 C 0.1363(13) 0.9609(7) 0.7908(5) 0.172(7) Uani 1 1 d . . . H92A H 0.2142 0.9728 0.7659 0.258 Uiso 1 1 calc R . . H92B H 0.1548 0.9239 0.8231 0.258 Uiso 1 1 calc R . . H92C H 0.0923 1.0041 0.8074 0.258 Uiso 1 1 calc R . . C93 C -0.0335(12) 0.9575(6) 0.6683(5) 0.124(4) Uani 1 1 d . . . H93A H -0.1169 0.9506 0.6910 0.149 Uiso 1 1 calc R . . H93B H 0.0046 0.9107 0.6551 0.149 Uiso 1 1 calc R . . C94 C -0.0468(10) 1.0092(6) 0.6168(4) 0.118(4) Uani 1 1 d . . . H94A H -0.0968 1.0531 0.6293 0.177 Uiso 1 1 calc R . . H94B H -0.0882 0.9886 0.5893 0.177 Uiso 1 1 calc R . . H94C H 0.0357 1.0209 0.5970 0.177 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0334(8) 0.0270(7) 0.0259(7) -0.0064(5) -0.0059(6) 0.0004(6) Ti2 0.0286(8) 0.0288(7) 0.0255(7) -0.0033(5) -0.0047(6) -0.0012(5) Ti3 0.0320(8) 0.0313(7) 0.0290(7) -0.0086(5) -0.0020(6) -0.0062(6) Ti4 0.0379(8) 0.0246(7) 0.0268(7) -0.0031(5) -0.0088(6) -0.0052(6) Si1 0.0252(11) 0.0297(11) 0.0269(10) -0.0041(8) -0.0063(9) -0.0002(8) Si2 0.0300(12) 0.0306(11) 0.0277(11) -0.0030(8) -0.0089(9) -0.0033(9) Si3 0.0339(12) 0.0226(10) 0.0257(10) -0.0029(8) -0.0032(9) -0.0021(8) Si4 0.0297(12) 0.0200(10) 0.0294(11) -0.0024(8) -0.0036(9) -0.0009(8) Cl1 0.0616(14) 0.0308(10) 0.0541(12) -0.0091(9) -0.0076(10) -0.0044(9) Cl2 0.0468(12) 0.0335(10) 0.0458(11) -0.0026(8) -0.0091(9) -0.0075(9) Cl3 0.0479(12) 0.0486(11) 0.0487(11) -0.0168(9) -0.0098(10) -0.0177(9) Cl4 0.0539(13) 0.0366(10) 0.0461(11) -0.0107(8) -0.0199(10) -0.0082(9) O1 0.029(3) 0.040(3) 0.023(2) -0.010(2) -0.005(2) 0.002(2) O2 0.027(3) 0.036(3) 0.026(2) -0.004(2) -0.003(2) -0.002(2) O3 0.035(3) 0.036(3) 0.022(2) -0.0016(19) -0.004(2) -0.001(2) O4 0.026(3) 0.032(3) 0.032(3) -0.007(2) -0.004(2) -0.003(2) O5 0.041(3) 0.026(2) 0.031(3) -0.0015(19) -0.008(2) -0.003(2) O6 0.043(3) 0.030(2) 0.018(2) -0.0012(19) -0.001(2) -0.006(2) O7 0.041(3) 0.019(2) 0.033(3) 0.0006(19) -0.001(2) 0.003(2) O8 0.033(3) 0.037(3) 0.022(2) -0.005(2) 0.000(2) -0.007(2) C1 0.029(4) 0.046(5) 0.027(4) -0.007(3) 0.003(3) -0.002(3) C2 0.035(5) 0.040(4) 0.032(4) -0.009(3) -0.001(3) 0.016(4) C3 0.030(4) 0.036(4) 0.026(4) -0.012(3) 0.005(3) 0.000(3) C4 0.030(4) 0.034(4) 0.029(4) -0.014(3) 0.006(3) 0.000(3) C5 0.030(4) 0.029(4) 0.026(4) -0.007(3) 0.010(3) -0.001(3) C6 0.032(5) 0.059(5) 0.040(4) -0.007(4) 0.006(4) -0.012(4) C7 0.048(5) 0.057(5) 0.050(5) -0.013(4) -0.013(4) 0.016(4) C8 0.092(7) 0.042(5) 0.027(4) -0.018(3) -0.007(4) 0.001(4) C9 0.044(5) 0.042(4) 0.031(4) -0.002(3) -0.007(4) -0.001(4) C10 0.047(5) 0.050(5) 0.045(5) -0.009(4) 0.003(4) -0.004(4) C11 0.029(4) 0.042(4) 0.027(4) 0.000(3) -0.008(3) -0.005(3) C12 0.035(5) 0.038(4) 0.028(4) -0.005(3) -0.004(3) -0.004(3) C13 0.036(5) 0.041(4) 0.027(4) 0.010(3) -0.007(4) -0.006(4) C14 0.035(5) 0.032(4) 0.023(4) -0.001(3) -0.006(3) -0.006(3) C15 0.032(4) 0.024(4) 0.026(4) -0.005(3) -0.013(3) 0.001(3) C16 0.039(5) 0.050(5) 0.043(4) -0.003(4) -0.008(4) -0.006(4) C17 0.072(6) 0.045(5) 0.036(4) -0.011(4) -0.009(4) -0.001(4) C18 0.039(5) 0.069(5) 0.038(5) 0.004(4) -0.006(4) -0.006(4) C19 0.033(5) 0.040(4) 0.052(5) 0.000(4) -0.013(4) -0.006(3) C20 0.044(5) 0.034(4) 0.045(4) -0.009(3) -0.019(4) 0.002(4) C21 0.033(5) 0.029(4) 0.035(4) 0.002(3) -0.014(4) 0.000(3) C22 0.026(4) 0.032(4) 0.056(5) -0.001(4) -0.011(4) -0.002(3) C23 0.040(5) 0.037(5) 0.070(6) 0.012(4) -0.010(4) -0.009(4) C24 0.043(6) 0.031(5) 0.109(8) 0.006(5) -0.030(6) -0.008(4) C25 0.074(7) 0.040(5) 0.081(7) -0.019(5) -0.033(6) 0.003(5) C26 0.058(6) 0.032(4) 0.050(5) 0.001(4) -0.024(4) -0.002(4) C27 0.020(4) 0.025(4) 0.024(4) 0.001(3) 0.001(3) -0.006(3) C28 0.035(5) 0.033(4) 0.034(4) 0.005(3) -0.004(3) -0.008(3) C29 0.062(6) 0.035(4) 0.032(4) -0.006(3) -0.003(4) -0.013(4) C30 0.056(6) 0.036(4) 0.046(5) -0.007(4) -0.003(4) 0.007(4) C31 0.038(5) 0.048(5) 0.044(5) 0.004(4) -0.013(4) 0.000(4) C32 0.039(5) 0.041(4) 0.035(4) -0.007(3) -0.001(4) -0.003(4) C33 0.042(5) 0.032(4) 0.023(4) 0.003(3) -0.009(3) -0.010(3) C34 0.035(5) 0.055(5) 0.033(4) -0.008(4) -0.005(4) -0.005(4) C35 0.037(5) 0.083(6) 0.041(5) -0.011(4) -0.008(4) -0.016(4) C36 0.071(7) 0.086(7) 0.036(5) -0.006(5) -0.021(5) -0.041(5) C37 0.085(7) 0.049(5) 0.049(5) -0.014(4) -0.021(5) -0.022(5) C38 0.053(5) 0.042(5) 0.030(4) 0.001(3) -0.017(4) -0.009(4) C39 0.026(4) 0.025(4) 0.034(4) -0.003(3) -0.001(3) 0.003(3) C40 0.036(5) 0.029(4) 0.041(4) -0.001(3) -0.006(4) 0.000(3) C41 0.045(5) 0.038(5) 0.053(5) -0.011(4) -0.006(4) -0.009(4) C42 0.053(6) 0.025(4) 0.081(6) -0.010(4) 0.007(5) -0.011(4) C43 0.059(6) 0.033(5) 0.044(5) 0.015(4) 0.008(4) -0.008(4) C44 0.044(5) 0.034(4) 0.035(4) -0.005(3) 0.001(4) 0.000(4) C45 0.034(5) 0.032(4) 0.035(4) -0.014(3) 0.009(4) -0.010(3) C46 0.023(4) 0.048(5) 0.032(4) -0.021(4) 0.012(3) -0.009(3) C47 0.031(5) 0.049(5) 0.023(4) -0.017(3) 0.006(3) -0.006(4) C48 0.035(5) 0.048(5) 0.034(4) -0.007(4) 0.003(4) -0.016(4) C49 0.028(5) 0.056(5) 0.035(4) -0.015(4) 0.004(4) -0.006(4) C50 0.035(5) 0.049(5) 0.060(5) -0.017(4) 0.001(4) 0.005(4) C51 0.038(5) 0.056(5) 0.049(5) -0.030(4) 0.006(4) -0.015(4) C52 0.049(6) 0.081(6) 0.038(5) -0.014(4) 0.003(4) -0.016(4) C53 0.055(6) 0.077(6) 0.049(5) 0.001(4) 0.002(4) -0.033(5) C54 0.035(5) 0.069(5) 0.055(5) -0.025(4) -0.011(4) -0.006(4) C55 0.042(5) 0.014(4) 0.048(5) 0.005(3) -0.009(4) -0.008(3) C56 0.062(6) 0.025(4) 0.032(4) 0.009(3) -0.012(4) -0.012(4) C57 0.067(6) 0.027(4) 0.043(5) 0.002(3) -0.030(5) -0.010(4) C58 0.048(5) 0.028(4) 0.039(4) -0.005(3) -0.015(4) 0.004(4) C59 0.055(6) 0.027(4) 0.022(4) 0.001(3) -0.010(4) -0.003(4) C60 0.069(6) 0.039(5) 0.041(5) 0.005(3) 0.001(4) -0.026(4) C61 0.117(8) 0.045(5) 0.027(4) 0.007(4) -0.018(5) -0.011(5) C62 0.054(6) 0.053(5) 0.090(6) -0.014(4) -0.036(5) 0.000(4) C63 0.056(6) 0.037(4) 0.041(5) -0.005(3) -0.007(4) 0.006(4) C64 0.052(5) 0.039(4) 0.046(4) -0.005(3) -0.021(4) -0.012(4) C65 0.030(4) 0.021(4) 0.029(4) -0.006(3) -0.004(3) 0.002(3) C66 0.040(5) 0.032(4) 0.037(4) -0.005(3) -0.003(4) -0.005(3) C67 0.061(6) 0.040(5) 0.045(5) -0.019(4) 0.022(5) -0.014(4) C68 0.031(5) 0.055(5) 0.082(7) -0.024(5) 0.010(5) -0.017(4) C69 0.047(6) 0.063(6) 0.058(6) -0.011(5) -0.014(5) -0.004(4) C70 0.038(5) 0.033(4) 0.036(4) 0.000(3) -0.002(4) -0.003(4) C71 0.048(5) 0.023(4) 0.026(4) 0.000(3) -0.005(4) -0.003(3) C72 0.049(5) 0.045(5) 0.040(4) -0.004(4) -0.013(4) -0.013(4) C73 0.074(7) 0.047(5) 0.057(6) 0.006(4) -0.027(5) -0.016(5) C74 0.093(8) 0.042(5) 0.045(5) 0.000(4) -0.034(5) -0.017(5) C75 0.087(7) 0.028(4) 0.028(4) -0.005(3) -0.003(4) -0.009(4) C76 0.071(6) 0.035(4) 0.031(4) -0.008(3) -0.008(4) -0.001(4) C77 0.025(4) 0.033(4) 0.027(4) 0.001(3) 0.001(3) -0.011(3) C78 0.039(5) 0.030(4) 0.040(4) -0.002(3) -0.003(4) -0.010(3) C79 0.036(5) 0.060(5) 0.032(4) -0.008(4) 0.000(4) -0.022(4) C80 0.054(5) 0.052(5) 0.045(5) -0.021(4) -0.011(4) -0.025(4) C81 0.062(6) 0.038(4) 0.048(5) -0.015(4) -0.002(4) -0.016(4) C82 0.037(5) 0.033(4) 0.041(4) -0.003(3) -0.002(4) -0.002(3) C83 0.038(4) 0.018(3) 0.025(4) -0.003(3) -0.007(3) -0.009(3) C84 0.039(5) 0.047(5) 0.042(5) 0.004(4) -0.007(4) -0.022(4) C85 0.061(6) 0.051(5) 0.037(5) 0.006(4) -0.007(4) -0.021(4) C86 0.064(6) 0.044(5) 0.058(6) 0.003(4) -0.036(5) 0.004(4) C87 0.044(5) 0.053(5) 0.055(5) 0.001(4) -0.016(5) -0.002(4) C88 0.035(5) 0.043(4) 0.035(4) -0.001(3) -0.006(4) -0.004(4) O9 0.110(6) 0.063(4) 0.082(5) -0.017(4) -0.025(4) -0.005(4) C91 0.169(14) 0.095(9) 0.098(9) 0.007(7) -0.019(9) -0.043(8) C92 0.205(16) 0.204(14) 0.113(10) -0.059(10) -0.090(11) 0.082(12) C93 0.148(13) 0.141(11) 0.102(9) -0.013(8) -0.026(9) -0.074(9) C94 0.098(10) 0.156(11) 0.113(9) 0.026(8) -0.034(8) -0.081(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.795(3) . ? Ti1 O4 1.816(4) . ? Ti1 Cl1 2.299(2) . ? Ti1 C5 2.323(7) . ? Ti1 C4 2.361(6) . ? Ti1 C1 2.368(7) . ? Ti1 C3 2.378(6) . ? Ti1 C2 2.401(6) . ? Ti2 O2 1.812(4) . ? Ti2 O1 1.817(4) . ? Ti2 Cl2 2.296(2) . ? Ti2 C14 2.326(6) . ? Ti2 C12 2.370(6) . ? Ti2 C15 2.372(5) . ? Ti2 C11 2.378(6) . ? Ti2 C13 2.381(7) . ? Ti3 O5 1.814(4) . ? Ti3 O8 1.819(4) . ? Ti3 Cl3 2.2841(19) . ? Ti3 C46 2.323(6) . ? Ti3 C45 2.358(6) . ? Ti3 C49 2.383(7) . ? Ti3 C47 2.389(6) . ? Ti3 C48 2.409(7) . ? Ti4 O6 1.810(4) . ? Ti4 O5 1.813(4) . ? Ti4 Cl4 2.2876(18) . ? Ti4 C59 2.338(6) . ? Ti4 C55 2.352(6) . ? Ti4 C58 2.375(6) . ? Ti4 C57 2.374(6) . ? Ti4 C56 2.378(6) . ? Si1 O2 1.617(4) . ? Si1 O3 1.618(4) . ? Si1 C27 1.857(6) . ? Si1 C21 1.859(7) . ? Si2 O3 1.633(4) . ? Si2 O4 1.637(4) . ? Si2 C39 1.846(6) . ? Si2 C33 1.854(6) . ? Si3 O7 1.613(4) . ? Si3 O6 1.626(4) . ? Si3 C65 1.825(7) . ? Si3 C71 1.872(6) . ? Si4 O7 1.629(4) . ? Si4 O8 1.633(4) . ? Si4 C83 1.855(6) . ? Si4 C77 1.863(6) . ? C1 C2 1.396(8) . ? C1 C5 1.419(8) . ? C1 C6 1.504(8) . ? C2 C3 1.431(8) . ? C2 C7 1.498(8) . ? C3 C4 1.396(7) . ? C3 C8 1.503(8) . ? C4 C5 1.404(7) . ? C4 C9 1.523(7) . ? C5 C10 1.499(8) . ? C11 C15 1.413(8) . ? C11 C12 1.414(8) . ? C11 C16 1.501(8) . ? C12 C13 1.412(9) . ? C12 C17 1.517(8) . ? C13 C14 1.428(8) . ? C13 C18 1.484(9) . ? C14 C15 1.417(8) . ? C14 C19 1.494(8) . ? C15 C20 1.477(8) . ? C21 C22 1.378(9) . ? C21 C26 1.394(8) . ? C22 C23 1.390(9) . ? C23 C24 1.362(9) . ? C24 C25 1.367(11) . ? C25 C26 1.362(10) . ? C27 C32 1.375(8) . ? C27 C28 1.396(7) . ? C28 C29 1.395(8) . ? C29 C30 1.372(9) . ? C30 C31 1.368(8) . ? C31 C32 1.378(8) . ? C33 C34 1.379(8) . ? C33 C38 1.396(8) . ? C34 C35 1.361(8) . ? C35 C36 1.367(9) . ? C36 C37 1.365(9) . ? C37 C38 1.390(8) . ? C39 C44 1.388(8) . ? C39 C40 1.406(8) . ? C40 C41 1.378(9) . ? C41 C42 1.364(9) . ? C42 C43 1.379(9) . ? C43 C44 1.380(9) . ? C45 C49 1.402(9) . ? C45 C46 1.428(8) . ? C45 C50 1.520(8) . ? C46 C47 1.406(9) . ? C46 C51 1.497(8) . ? C47 C48 1.425(9) . ? C47 C52 1.501(8) . ? C48 C49 1.397(8) . ? C48 C53 1.488(9) . ? C49 C54 1.517(8) . ? C55 C56 1.398(9) . ? C55 C59 1.407(8) . ? C55 C60 1.501(9) . ? C56 C57 1.420(10) . ? C56 C61 1.490(8) . ? C57 C58 1.426(8) . ? C57 C62 1.507(9) . ? C58 C59 1.411(9) . ? C58 C63 1.496(9) . ? C59 C64 1.511(8) . ? C65 C66 1.396(8) . ? C65 C70 1.400(8) . ? C66 C67 1.386(9) . ? C67 C68 1.370(9) . ? C68 C69 1.358(10) . ? C69 C70 1.372(10) . ? C71 C76 1.382(8) . ? C71 C72 1.385(9) . ? C72 C73 1.389(9) . ? C73 C74 1.357(10) . ? C74 C75 1.382(10) . ? C75 C76 1.409(9) . ? C77 C78 1.400(8) . ? C77 C82 1.404(8) . ? C78 C79 1.375(8) . ? C79 C80 1.379(8) . ? C80 C81 1.385(9) . ? C81 C82 1.379(8) . ? C83 C84 1.377(9) . ? C83 C88 1.383(8) . ? C84 C85 1.391(8) . ? C85 C86 1.374(10) . ? C86 C87 1.376(10) . ? C87 C88 1.401(8) . ? O9 C93 1.379(10) . ? O9 C91 1.388(10) . ? C91 C92 1.433(13) . ? C93 C94 1.448(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O4 105.59(17) . . ? O1 Ti1 Cl1 101.83(14) . . ? O4 Ti1 Cl1 102.21(14) . . ? O1 Ti1 C5 101.5(2) . . ? O4 Ti1 C5 96.8(2) . . ? Cl1 Ti1 C5 144.53(15) . . ? O1 Ti1 C4 136.3(2) . . ? O4 Ti1 C4 87.5(2) . . ? Cl1 Ti1 C4 116.14(15) . . ? C5 Ti1 C4 34.88(19) . . ? O1 Ti1 C1 84.3(2) . . ? O4 Ti1 C1 131.3(2) . . ? Cl1 Ti1 C1 122.60(17) . . ? C5 Ti1 C1 35.19(19) . . ? C4 Ti1 C1 57.7(2) . . ? O1 Ti1 C3 137.8(2) . . ? O4 Ti1 C3 112.55(19) . . ? Cl1 Ti1 C3 87.38(17) . . ? C5 Ti1 C3 57.6(2) . . ? C4 Ti1 C3 34.26(18) . . ? C1 Ti1 C3 57.2(2) . . ? O1 Ti1 C2 103.28(19) . . ? O4 Ti1 C2 144.9(2) . . ? Cl1 Ti1 C2 90.83(18) . . ? C5 Ti1 C2 57.9(2) . . ? C4 Ti1 C2 57.7(2) . . ? C1 Ti1 C2 34.0(2) . . ? C3 Ti1 C2 34.84(19) . . ? O2 Ti2 O1 105.11(16) . . ? O2 Ti2 Cl2 103.42(14) . . ? O1 Ti2 Cl2 101.85(15) . . ? O2 Ti2 C14 98.5(2) . . ? O1 Ti2 C14 97.5(2) . . ? Cl2 Ti2 C14 145.69(16) . . ? O2 Ti2 C12 108.0(2) . . ? O1 Ti2 C12 141.27(19) . . ? Cl2 Ti2 C12 89.60(17) . . ? C14 Ti2 C12 58.4(2) . . ? O2 Ti2 C15 133.5(2) . . ? O1 Ti2 C15 84.57(18) . . ? Cl2 Ti2 C15 119.25(16) . . ? C14 Ti2 C15 35.1(2) . . ? C12 Ti2 C15 58.01(19) . . ? O2 Ti2 C11 141.4(2) . . ? O1 Ti2 C11 107.87(19) . . ? Cl2 Ti2 C11 89.05(17) . . ? C14 Ti2 C11 57.9(2) . . ? C12 Ti2 C11 34.6(2) . . ? C15 Ti2 C11 34.60(19) . . ? O2 Ti2 C13 85.4(2) . . ? O1 Ti2 C13 132.7(2) . . ? Cl2 Ti2 C13 120.74(17) . . ? C14 Ti2 C13 35.3(2) . . ? C12 Ti2 C13 34.6(2) . . ? C15 Ti2 C13 58.1(2) . . ? C11 Ti2 C13 57.4(2) . . ? O5 Ti3 O8 105.4(2) . . ? O5 Ti3 Cl3 100.97(13) . . ? O8 Ti3 Cl3 103.93(13) . . ? O5 Ti3 C46 97.9(2) . . ? O8 Ti3 C46 100.4(2) . . ? Cl3 Ti3 C46 143.80(19) . . ? O5 Ti3 C45 133.4(2) . . ? O8 Ti3 C45 86.7(2) . . ? Cl3 Ti3 C45 119.90(18) . . ? C46 Ti3 C45 35.5(2) . . ? O5 Ti3 C49 140.4(2) . . ? O8 Ti3 C49 109.3(2) . . ? Cl3 Ti3 C49 88.78(17) . . ? C46 Ti3 C49 57.7(2) . . ? C45 Ti3 C49 34.4(2) . . ? O5 Ti3 C47 85.0(2) . . ? O8 Ti3 C47 135.0(2) . . ? Cl3 Ti3 C47 117.17(19) . . ? C46 Ti3 C47 34.7(2) . . ? C45 Ti3 C47 57.9(2) . . ? C49 Ti3 C47 57.0(2) . . ? O5 Ti3 C48 107.7(2) . . ? O8 Ti3 C48 142.3(2) . . ? Cl3 Ti3 C48 87.03(17) . . ? C46 Ti3 C48 57.8(2) . . ? C45 Ti3 C48 57.4(2) . . ? C49 Ti3 C48 33.9(2) . . ? C47 Ti3 C48 34.6(2) . . ? O6 Ti4 O5 105.76(18) . . ? O6 Ti4 Cl4 103.47(14) . . ? O5 Ti4 Cl4 101.74(13) . . ? O6 Ti4 C59 96.5(2) . . ? O5 Ti4 C59 100.5(2) . . ? Cl4 Ti4 C59 144.60(16) . . ? O6 Ti4 C55 131.1(2) . . ? O5 Ti4 C55 85.1(2) . . ? Cl4 Ti4 C55 121.11(17) . . ? C59 Ti4 C55 34.9(2) . . ? O6 Ti4 C58 85.5(2) . . ? O5 Ti4 C58 135.3(2) . . ? Cl4 Ti4 C58 117.78(17) . . ? C59 Ti4 C58 34.8(2) . . ? C55 Ti4 C58 57.6(3) . . ? O6 Ti4 C57 110.2(2) . . ? O5 Ti4 C57 139.5(3) . . ? Cl4 Ti4 C57 87.54(16) . . ? C59 Ti4 C57 58.0(2) . . ? C55 Ti4 C57 57.3(2) . . ? C58 Ti4 C57 34.96(19) . . ? O6 Ti4 C56 142.9(2) . . ? O5 Ti4 C56 105.3(2) . . ? Cl4 Ti4 C56 89.48(17) . . ? C59 Ti4 C56 58.1(2) . . ? C55 Ti4 C56 34.4(2) . . ? C58 Ti4 C56 58.1(2) . . ? C57 Ti4 C56 34.8(2) . . ? O2 Si1 O3 109.6(2) . . ? O2 Si1 C27 108.9(2) . . ? O3 Si1 C27 109.3(2) . . ? O2 Si1 C21 110.8(2) . . ? O3 Si1 C21 108.2(2) . . ? C27 Si1 C21 110.1(3) . . ? O3 Si2 O4 110.4(2) . . ? O3 Si2 C39 106.8(2) . . ? O4 Si2 C39 110.6(3) . . ? O3 Si2 C33 107.5(3) . . ? O4 Si2 C33 108.9(2) . . ? C39 Si2 C33 112.6(3) . . ? O7 Si3 O6 109.6(2) . . ? O7 Si3 C65 107.6(2) . . ? O6 Si3 C65 109.9(2) . . ? O7 Si3 C71 107.4(2) . . ? O6 Si3 C71 110.3(3) . . ? C65 Si3 C71 112.0(3) . . ? O7 Si4 O8 109.4(2) . . ? O7 Si4 C83 108.6(2) . . ? O8 Si4 C83 110.2(3) . . ? O7 Si4 C77 106.6(3) . . ? O8 Si4 C77 111.0(2) . . ? C83 Si4 C77 110.9(3) . . ? Ti1 O1 Ti2 149.6(2) . . ? Si1 O2 Ti2 164.7(2) . . ? Si1 O3 Si2 146.5(3) . . ? Si2 O4 Ti1 166.7(2) . . ? Ti4 O5 Ti3 151.3(2) . . ? Si3 O6 Ti4 162.6(3) . . ? Si3 O7 Si4 149.1(3) . . ? Si4 O8 Ti3 159.9(2) . . ? C2 C1 C5 108.7(5) . . ? C2 C1 C6 126.8(6) . . ? C5 C1 C6 124.4(6) . . ? C2 C1 Ti1 74.3(4) . . ? C5 C1 Ti1 70.7(4) . . ? C6 C1 Ti1 123.8(4) . . ? C1 C2 C3 106.8(5) . . ? C1 C2 C7 125.8(6) . . ? C3 C2 C7 127.3(6) . . ? C1 C2 Ti1 71.7(4) . . ? C3 C2 Ti1 71.7(4) . . ? C7 C2 Ti1 123.9(5) . . ? C4 C3 C2 108.7(5) . . ? C4 C3 C8 127.2(5) . . ? C2 C3 C8 124.0(6) . . ? C4 C3 Ti1 72.2(3) . . ? C2 C3 Ti1 73.4(3) . . ? C8 C3 Ti1 123.9(5) . . ? C3 C4 C5 107.9(5) . . ? C3 C4 C9 125.3(5) . . ? C5 C4 C9 126.7(5) . . ? C3 C4 Ti1 73.6(4) . . ? C5 C4 Ti1 71.1(4) . . ? C9 C4 Ti1 121.9(4) . . ? C4 C5 C1 107.9(5) . . ? C4 C5 C10 127.1(5) . . ? C1 C5 C10 124.9(6) . . ? C4 C5 Ti1 74.0(4) . . ? C1 C5 Ti1 74.1(4) . . ? C10 C5 Ti1 121.3(4) . . ? C15 C11 C12 108.9(6) . . ? C15 C11 C16 126.2(6) . . ? C12 C11 C16 124.9(6) . . ? C15 C11 Ti2 72.5(3) . . ? C12 C11 Ti2 72.3(3) . . ? C16 C11 Ti2 123.3(4) . . ? C13 C12 C11 108.0(6) . . ? C13 C12 C17 125.3(6) . . ? C11 C12 C17 126.7(6) . . ? C13 C12 Ti2 73.1(3) . . ? C11 C12 Ti2 73.0(3) . . ? C17 C12 Ti2 122.5(4) . . ? C12 C13 C14 107.5(6) . . ? C12 C13 C18 127.1(6) . . ? C14 C13 C18 125.4(6) . . ? C12 C13 Ti2 72.3(4) . . ? C14 C13 Ti2 70.2(4) . . ? C18 C13 Ti2 122.4(4) . . ? C15 C14 C13 108.3(5) . . ? C15 C14 C19 125.5(5) . . ? C13 C14 C19 126.0(6) . . ? C15 C14 Ti2 74.2(4) . . ? C13 C14 Ti2 74.5(4) . . ? C19 C14 Ti2 121.8(4) . . ? C11 C15 C14 107.2(5) . . ? C11 C15 C20 127.4(6) . . ? C14 C15 C20 125.4(5) . . ? C11 C15 Ti2 72.9(3) . . ? C14 C15 Ti2 70.7(3) . . ? C20 C15 Ti2 123.4(4) . . ? C22 C21 C26 117.1(6) . . ? C22 C21 Si1 121.5(5) . . ? C26 C21 Si1 121.4(6) . . ? C21 C22 C23 121.3(7) . . ? C24 C23 C22 119.8(8) . . ? C23 C24 C25 119.9(8) . . ? C26 C25 C24 120.5(8) . . ? C25 C26 C21 121.4(8) . . ? C32 C27 C28 118.5(5) . . ? C32 C27 Si1 120.5(4) . . ? C28 C27 Si1 121.0(5) . . ? C29 C28 C27 119.4(6) . . ? C30 C29 C28 121.1(6) . . ? C31 C30 C29 118.9(6) . . ? C30 C31 C32 120.8(7) . . ? C27 C32 C31 121.1(6) . . ? C34 C33 C38 116.3(6) . . ? C34 C33 Si2 121.6(5) . . ? C38 C33 Si2 121.9(5) . . ? C35 C34 C33 123.1(6) . . ? C34 C35 C36 119.6(7) . . ? C37 C36 C35 120.0(7) . . ? C36 C37 C38 119.9(7) . . ? C37 C38 C33 121.0(6) . . ? C44 C39 C40 116.4(6) . . ? C44 C39 Si2 123.8(5) . . ? C40 C39 Si2 119.8(5) . . ? C41 C40 C39 121.7(6) . . ? C42 C41 C40 120.4(7) . . ? C41 C42 C43 119.4(7) . . ? C42 C43 C44 120.4(7) . . ? C43 C44 C39 121.7(6) . . ? C49 C45 C46 106.8(6) . . ? C49 C45 C50 126.1(6) . . ? C46 C45 C50 127.0(6) . . ? C49 C45 Ti3 73.8(4) . . ? C46 C45 Ti3 70.9(3) . . ? C50 C45 Ti3 121.3(4) . . ? C47 C46 C45 108.2(6) . . ? C47 C46 C51 125.4(6) . . ? C45 C46 C51 126.3(7) . . ? C47 C46 Ti3 75.2(3) . . ? C45 C46 Ti3 73.6(3) . . ? C51 C46 Ti3 120.6(4) . . ? C46 C47 C48 107.8(6) . . ? C46 C47 C52 124.5(6) . . ? C48 C47 C52 127.7(7) . . ? C46 C47 Ti3 70.1(3) . . ? C48 C47 Ti3 73.5(4) . . ? C52 C47 Ti3 123.2(4) . . ? C49 C48 C47 107.4(6) . . ? C49 C48 C53 127.2(6) . . ? C47 C48 C53 125.3(6) . . ? C49 C48 Ti3 72.0(4) . . ? C47 C48 Ti3 71.9(4) . . ? C53 C48 Ti3 124.1(5) . . ? C48 C49 C45 109.7(6) . . ? C48 C49 C54 125.8(7) . . ? C45 C49 C54 124.4(7) . . ? C48 C49 Ti3 74.1(4) . . ? C45 C49 Ti3 71.8(4) . . ? C54 C49 Ti3 123.3(4) . . ? C56 C55 C59 109.5(7) . . ? C56 C55 C60 125.5(7) . . ? C59 C55 C60 125.1(6) . . ? C56 C55 Ti4 73.8(4) . . ? C59 C55 Ti4 72.0(4) . . ? C60 C55 Ti4 121.5(4) . . ? C55 C56 C57 107.1(6) . . ? C55 C56 C61 127.3(8) . . ? C57 C56 C61 125.6(7) . . ? C55 C56 Ti4 71.8(4) . . ? C57 C56 Ti4 72.5(4) . . ? C61 C56 Ti4 123.0(4) . . ? C56 C57 C58 108.3(6) . . ? C56 C57 C62 126.2(6) . . ? C58 C57 C62 125.5(7) . . ? C56 C57 Ti4 72.8(4) . . ? C58 C57 Ti4 72.5(3) . . ? C62 C57 Ti4 122.2(5) . . ? C59 C58 C57 107.2(6) . . ? C59 C58 C63 127.6(6) . . ? C57 C58 C63 125.2(7) . . ? C59 C58 Ti4 71.1(3) . . ? C57 C58 Ti4 72.5(3) . . ? C63 C58 Ti4 122.0(4) . . ? C55 C59 C58 107.9(6) . . ? C55 C59 C64 125.8(7) . . ? C58 C59 C64 126.2(6) . . ? C55 C59 Ti4 73.1(3) . . ? C58 C59 Ti4 74.0(4) . . ? C64 C59 Ti4 121.0(4) . . ? C66 C65 C70 116.0(6) . . ? C66 C65 Si3 120.3(5) . . ? C70 C65 Si3 123.4(5) . . ? C67 C66 C65 121.5(6) . . ? C68 C67 C66 120.6(7) . . ? C69 C68 C67 118.8(8) . . ? C68 C69 C70 121.5(7) . . ? C69 C70 C65 121.5(7) . . ? C76 C71 C72 118.6(6) . . ? C76 C71 Si3 122.0(6) . . ? C72 C71 Si3 119.2(5) . . ? C71 C72 C73 121.9(7) . . ? C74 C73 C72 118.7(8) . . ? C73 C74 C75 121.7(7) . . ? C74 C75 C76 119.1(7) . . ? C71 C76 C75 120.0(7) . . ? C78 C77 C82 116.9(6) . . ? C78 C77 Si4 121.0(5) . . ? C82 C77 Si4 122.0(5) . . ? C79 C78 C77 120.5(6) . . ? C78 C79 C80 122.0(6) . . ? C79 C80 C81 118.6(6) . . ? C82 C81 C80 120.0(6) . . ? C81 C82 C77 122.0(6) . . ? C84 C83 C88 117.7(6) . . ? C84 C83 Si4 119.9(5) . . ? C88 C83 Si4 122.4(5) . . ? C83 C84 C85 122.2(7) . . ? C86 C85 C84 119.4(7) . . ? C85 C86 C87 119.9(7) . . ? C86 C87 C88 120.0(7) . . ? C83 C88 C87 120.9(7) . . ? C93 O9 C91 117.7(8) . . ? O9 C91 C92 114.1(10) . . ? O9 C93 C94 112.1(9) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.402 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.093